CN218130473U - Device for preparing polymeric ferric sulfate by using waste battery electrolyte - Google Patents

Device for preparing polymeric ferric sulfate by using waste battery electrolyte Download PDF

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CN218130473U
CN218130473U CN202221269431.4U CN202221269431U CN218130473U CN 218130473 U CN218130473 U CN 218130473U CN 202221269431 U CN202221269431 U CN 202221269431U CN 218130473 U CN218130473 U CN 218130473U
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ferric sulfate
polymeric ferric
electrolyte
sulfate
reaction kettle
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杨海涛
沈煜婷
李博洋
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Jiangsu Haibao Resources Recycling Technology Co ltd
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Jiangsu Haibao Resources Recycling Technology Co ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/84Recycling of batteries or fuel cells

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Abstract

The utility model discloses an utilize old and useless battery electrolyte to prepare polymeric ferric sulfate's device, including electrolyte collecting vessel, ferric sulfate polymerization cauldron and the solid polymeric ferric sulfate storage tank that sets gradually, still include purification dilute sulphuric acid storage bucket, pressure filter, evaporation enrichment reation kettle I, cooling tank I and microfilter have connected gradually between electrolyte collecting vessel and the purification dilute sulphuric acid storage bucket, be equipped with ferrous sulfate preparation reation kettle between purification dilute sulphuric acid storage bucket and the ferric sulfate polymerization cauldron, ferrous sulfate preparation reation kettle links to each other with evaporation enrichment reation kettle II, cooling tank II and centrifuge in proper order. The utility model discloses greatly promoted validity and the sufficiency to the utilization of dilute sulphuric acid electrolyte, and when promoting whole preparation process's accurate nature and stability by a wide margin, greatly improved the purity of the polyferric sulfate who makes.

Description

Device for preparing polymeric ferric sulfate by using waste battery electrolyte
Technical Field
The utility model relates to a lead acid battery recycle technical field specifically says, relates to an utilize old and useless battery electrolyte to prepare polymeric ferric sulfate's device.
Background
The service life of a lead-acid storage battery is generally 1-3 years, thousands of tons of waste batteries are generated every year, the main components of the lead-acid storage battery are lead, ABS/PE plastics, a partition plate and dilute sulfuric acid electrolyte, wherein the lead and ABS/PE plastics can be recycled through smelting, the partition plate is converted into furnace slag in the smelting process, the electrolyte occupying 15-25% of the weight of the waste batteries is generally neutralized by slaked lime to prepare calcium sulfate, the calcium sulfate is treated as common solid waste, and sodium sulfate and other products are prepared by manufacturers.
In order to solve the problems, the Chinese patent publication No. CN212387742U discloses a device for preparing polymeric ferric sulfate from lead smelting waste residues, and proposes that the device comprises a dilute acid storage tank, a dilute acid output pump, a waste residue pickling tank, a plate-and-frame booster pump, a plate-and-frame filter press, a plate-and-frame product tank, a heat exchanger, a nanofiltration membrane booster pump, a nanofiltration membrane group, a nanofiltration product tank, a reaction kettle feeding pump, a ferric sulfate polymerization reaction kettle, a spiral discharging machine and a solid polymeric ferric sulfate storage tank which are sequentially connected through a pipeline, wherein a storage battery acid pouring machine is used for collecting electrolyte of a waste lead acid storage battery and storing the electrolyte in the dilute acid storage tank, the ferric sulfate polymerization reaction kettle is provided with a heating system, an oxidant automatic dosing tank is configured, and a spray dryer is arranged at a discharge hole.
Although the prior art realizes preparation of the electrolyte in the waste battery into the polymeric ferric sulfate to a certain extent, the plate-and-frame filter press in the prior art has the function of filter pressing of solutions such as ferric sulfate in waste residue pickling, does not comprise equipment for purifying the collected dilute sulfuric acid electrolyte of the waste battery before the waste residue pickling, has limited effectiveness and sufficiency for utilization of the dilute sulfuric acid electrolyte of the waste battery, and is used for purifying and filtering the dilute sulfuric acid electrolyte directly prepared into the solutions such as ferric sulfate by the waste residue pickling tank through equipment such as the plate-and-frame filter press and a nanofiltration membrane group, the preparation process before the polymeric ferric sulfate is too extensive, and the by-products in the preparation process are easily generated by filtering after reaction, so that the purity of the prepared polymeric ferric sulfate is finally influenced.
For this reason, a new technical solution is needed to solve the above technical problems.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide an utilize waste battery electrolyte to prepare polyferric sulfate's device to solve the current device that utilizes waste battery electrolyte to prepare polyferric sulfate that above-mentioned background art provided, it is limited to validity and sufficiency that electrolyte utilized, and the preparation process before the polyferric sulfate of polymerization is too extensive simultaneously, and for the prefilter that reacts earlier, the also general technical problem of purity of the polyferric sulfate that finally makes.
In order to achieve the purpose, the utility model adopts the following technical proposal:
a device for preparing polyferric sulfate by using waste battery electrolyte comprises an electrolyte collecting barrel, a purified dilute sulfuric acid storage barrel, a ferric sulfate polymerization reaction kettle and a solid polyferric sulfate storage tank which are sequentially arranged, wherein a pressure filter, an evaporation and enrichment reaction kettle I, a cooling pool I and a microfilter are sequentially connected between the electrolyte collecting barrel and the purified dilute sulfuric acid storage barrel, an electrolyte storage tank is connected between the pressure filter and the evaporation and enrichment reaction kettle I, a ferrous sulfate preparation reaction kettle, an evaporation and enrichment reaction kettle II, a cooling pool II and a centrifugal machine are sequentially arranged between the purified dilute sulfuric acid storage barrel and the ferric sulfate polymerization reaction kettle, the ferrous sulfate preparation reaction kettle, the evaporation and enrichment reaction kettle II, the cooling pool II and the centrifugal machine are sequentially connected, a ferrous sulfate solution storage tank is connected between the ferrous sulfate preparation reaction kettle and the evaporation and enrichment reaction kettle II, a polyferric sulfate solution storage tank, a polyferric sulfate atomization drying box and a solid polyferric sulfate collecting box are sequentially connected between the solid polyferric sulfate collecting box and the solid polyferric sulfate collecting box, a conveying auger is connected between the solid polyferric sulfate collecting box and the solid polyferric sulfate collecting box, the polyferric sulfate atomization drying box is further connected with an air collecting box, a negative pressure fan is connected between the solid polyferric sulfate collecting box;
furthermore, a polymeric ferric sulfate solution pump-out pipeline is arranged between the ferric sulfate polymerization reaction kettle and the polymeric ferric sulfate solution storage tank, the ferric sulfate polymerization reaction kettle and the polymeric ferric sulfate solution storage tank are connected through the polymeric ferric sulfate solution pump-out pipeline, a circulating pipeline is further connected in parallel to the polymeric ferric sulfate solution pump-out pipeline, the circulating pipeline is simultaneously connected with the ferric sulfate polymerization reaction kettle, an oxygen pump inlet, a sodium nitrite solution pump inlet and a charging opening are arranged on the ferric sulfate polymerization reaction kettle, and a pressure gauge is further installed on the ferric sulfate polymerization reaction kettle.
Compared with the prior art, the beneficial effects of the utility model are that:
1. the utility model discloses in through addding purification dilute sulphuric acid storage bucket, and the pressure filter that connects gradually between electrolyte collecting vessel and purification dilute sulphuric acid storage bucket, evaporation enrichment reation kettle I, the cooperation setting of cooling bath I and microfilter, with the mode that evaporation enrichment adds the micro-filtration, with the concentration of the dilute sulphuric acid electrolyte that the electrolyte collecting vessel was collected, before being used for in ferrous sulfate preparation reation kettle, carry out purification promotion in advance, obtain purification dilute sulphuric acid, greatly promoted validity and sufficiency to the utilization of dilute sulphuric acid electrolyte, on this basis, earlier through the cooperation setting of ferrous sulfate preparation reation kettle, utilize purification dilute sulphuric acid to prepare and obtain ferrous sulfate solution, rethread evaporation enrichment reation kettle II, the cooperation setting of cooling bath II and centrifuge, with the mode that evaporation enrichment adds the cooling centrifugation, purify the promotion to the concentration of ferrous sulfate, and obtain the solid ferrous sulfate after the purification, carry out polymerization again, when promoting whole preparation process's precision and stability by a wide margin, the purity of the polyferric sulfate that makes has greatly improved;
2. the utility model discloses in filter through the dilute sulphuric acid electrolyte that utilizes the pressure filter to collect the electrolyte collecting vessel, filter solid particle wherein, then shift it to evaporation enrichment reation kettle I, enrich to the settlement concentration, shift to cooling tank I cooling back again, filter through the microfilter and separate out the insoluble substance, finally can obtain the clarification dilute sulphuric acid (being purification dilute sulphuric acid) of settlement concentration to store in purification dilute sulphuric acid storage bucket, thereby further guaranteed effectively validity and the sufficiency to the utilization of dilute sulphuric acid electrolyte;
3. the utility model discloses in the cooperation setting through the oxygen pump entry on the ferric sulfate polymerization cauldron and the manometer, utilize the pressure state to in the ferric sulfate polymerization cauldron to monitor, in time feed back polymerization's the beginning and the end state to the output time of reasonable adjustment oxygen has further promoted accurate nature and the stability of whole preparation process.
Drawings
Fig. 1 is a first schematic diagram of the working process of the present invention;
fig. 2 is a schematic diagram of the work flow of the present invention;
fig. 3 is a third schematic view of the work flow of the present invention;
fig. 4 is a schematic view of the working principle of the embodiment of the present invention;
in the figure: 1. an electrolyte collecting barrel, 2, a filter press, 3, an electrolyte storage tank, 4, an evaporation enrichment reaction kettle I, 5, a cooling pool I, 6, a micro filter, 7, a purified dilute sulfuric acid storage barrel, 8, a ferrous sulfate preparation reaction kettle, 9, a ferrous sulfate solution storage tank, 10, an evaporation enrichment reaction kettle II, 11, a cooling pool II, 12, a conveying auger II, 13, a centrifugal machine, 14, a ferric sulfate polymerization reaction kettle, 15, a charging opening, 16, a sodium nitrite solution pump inlet, 17, an oxygen pump inlet, 18, a pressure gauge, 19, a circulating pipeline, 20, a polymeric ferric sulfate solution pump-out pipeline, 21, a polymeric ferric sulfate solution storage tank, 22, an air heater, 23, a polymeric ferric sulfate atomization drying box, 24, a solid polymeric ferric sulfate collecting box, 25, a negative pressure fan, 26, a conveying auger I, 27, a solid polymeric ferric sulfate storage tank, 28 and a bag filling opening.
Detailed Description
The following examples are intended to further illustrate the invention and are not intended to limit its application.
Referring to fig. 1 to 4, a device for preparing polyferric sulfate by using a waste battery electrolyte is shown, which includes an electrolyte collecting barrel 1, a purified dilute sulfuric acid storage barrel 7, a ferrous sulfate preparation reaction kettle 8, a ferric sulfate polymerization reaction 14 and a solid polyferric sulfate storage tank 27, which are sequentially arranged according to a preparation process sequence, wherein a filter press 2, an electrolyte storage tank 3, an evaporation enrichment reaction kettle i 4, a cooling tank i 5 and a microfilter 6 are sequentially connected between the electrolyte collecting barrel 1 and the purified dilute sulfuric acid storage barrel 7 through pipelines, a ferrous sulfate solution storage tank 9, an evaporation enrichment reaction kettle ii 10, a cooling tank ii 11, a conveying auger ii 12 and a centrifuge 13 are sequentially arranged between the ferrous sulfate preparation reaction kettle 8 and the ferric sulfate polymerization reaction 14 according to the preparation process sequence, the ferrous sulfate preparation reaction kettle 8 is sequentially connected with the ferrous sulfate solution storage tank 9, the evaporation enrichment reaction kettle ii 10 and the cooling tank ii 11 through pipelines, the cooling tank ii 11 and the centrifuge 13 are connected through a conveying auger 12, a polyferric sulfate solution collecting tank 21, an atomization drying box 23 and a polyferric sulfate polymerization reaction solution 24 are sequentially connected between the ferric sulfate polymerization reaction kettle 14 and the solid polyferric sulfate polymerization reaction tank 14 through a pipeline 26, and the polyferric sulfate solution collecting tank 24, which are sequentially connected through pipelines;
furthermore, a circulating pipeline 19 connected with the ferric sulfate polymerization reaction kettle 14 is connected in parallel on the polymeric ferric sulfate solution pumping-out pipeline 20, the polymeric ferric sulfate atomization drying box 23 is simultaneously connected with an air heater 22, the solid polymeric ferric sulfate collection box 24 is simultaneously connected with a negative pressure fan 25, and the solid polymeric ferric sulfate storage tank 27 is provided with a bag filling opening 28; wherein, the ferric sulfate polymerization reaction kettle 14 is provided with a charging opening 15, a sodium nitrite solution pump inlet 16 and an oxygen pump inlet 17, and is provided with a pressure gauge 18.
The method for preparing the polymeric ferric sulfate by using the device of the utility model comprises the following steps:
s1, enriching and removing impurities from the waste battery electrolyte to prepare purified dilute sulfuric acid with the concentration of 35 percent:
the collected electrolyte of the waste battery is stored in an electrolyte collecting barrel 1 in a centralized manner, solid particles in the electrolyte collected by the electrolyte collecting barrel 1 are filtered by a filter press, then transferred to an evaporation and enrichment reaction kettle I4 in batches for heating and evaporation until the concentration of dilute sulfuric acid is enriched to 35%, transferred to a cooling pool I5 for cooling, and then filtered out insoluble substances separated out by a micro filter 6, so that purified dilute sulfuric acid (clarified dilute sulfuric acid) with the concentration of 35% can be finally obtained, and the purified dilute sulfuric acid is stored in a purified dilute sulfuric acid storage barrel 7 for later use;
s2, preparing solid ferrous sulfate by using purified dilute sulfuric acid with the concentration of 35%:
adding the purified dilute sulfuric acid with the concentration of 35% prepared in the step S1 into a ferrous sulfate preparation reaction kettle 8 (the adding amount of the purified dilute sulfuric acid is not more than 80% of the volume of the ferrous sulfate preparation reaction kettle 8), adding excessive iron filings into the ferrous sulfate preparation reaction kettle 8 in batches (the iron filings are cleaned by using alkali liquor before being added to remove oil stains), controlling the temperature in the ferrous sulfate preparation reaction kettle 8 to be between 50 and 70 ℃, accelerating the reaction speed by using a stirring mechanism of the ferrous sulfate preparation reaction kettle 8, transferring the prepared ferrous sulfate solution into a ferrous sulfate solution storage tank 9 for storage when no obvious bubbles are generated on the surface of the iron filings or the pH value of the solution in the ferrous sulfate preparation reaction kettle 8 is more than 1, then adding the prepared ferrous sulfate solution into an evaporation enrichment reaction kettle II 10 in batches for evaporation and enrichment (stirring in the evaporation process), transferring the prepared ferrous sulfate solution into a cooling pool II 11 for cooling when the solid-liquid temperature is reduced to be below 30 ℃, transferring the ferrous sulfate mixture in a solid-liquid storage tank II 12 to a centrifuge 13, and returning the solid-liquid solution to the centrifuge 13 after the solid-liquid separation by the centrifuge II 13;
s3, preparing solid polyferric sulfate by using purified dilute sulfuric acid with the concentration of 35% and ferrous sulfate:
firstly, adding 1 part of purified dilute sulfuric acid with the concentration of 35% into a ferric sulfate polymerization reaction kettle 14 through a feeding port 15, then starting a circulating system of the ferric sulfate polymerization reaction kettle 14, enabling the solution in the ferric sulfate polymerization reaction kettle 14 to circulate from bottom to top outside through a circulating pipeline 19, adding 1.5 parts of ferrous sulfate into the ferric sulfate polymerization reaction kettle 14 through the feeding port 15, heating the ferric sulfate polymerization reaction kettle 14 to control the temperature of the ferric sulfate polymerization reaction kettle to be 50-70 ℃, simultaneously adding 0.2 part of sodium nitrite solution with the concentration of 30% into the ferric sulfate polymerization reaction kettle 14 by 5 times through a sodium nitrite solution pump inlet 16, adding oxygen through an oxygen pump inlet 17, when the pressure of a pressure gauge 18 is 0.85MPa, carrying out oxidative polymerization reaction in the ferric sulfate polymerization reaction kettle 14 to generate liquid polymeric ferric sulfate, when the pressure of the pressure gauge 18 is reduced to be below 0.05MPa, finishing the reaction, sampling and testing the ferrous ion content to meet the requirement, pumping out pumping and transferring the liquid polymeric ferric sulfate solution 21 to a polymeric ferric sulfate storage tank through a polymeric sulfate solution pump outlet 20;
and secondly, starting a negative pressure fan 25, starting heating in the polymeric ferric sulfate atomizing and drying box 23 through the high-power air heater 22, measuring that the temperature in the polymeric ferric sulfate atomizing and drying box 23 reaches 120-130 ℃, starting an atomizing nozzle of the polymeric ferric sulfate atomizing and drying box 23, rapidly vaporizing the atomized particles of the polymeric ferric sulfate at high temperature to form water vapor and powdery solid polymeric ferric sulfate, and reaching the solid polymeric ferric sulfate collecting box 24 along with the air flow, settling the powdery solid polymeric ferric sulfate at the bottom of the solid polymeric ferric sulfate collecting box 24, conveying the solid polymeric ferric sulfate to a ferric sulfate polymeric storage tank 27 through a conveying auger I26 for storage, discharging the solid polymeric ferric sulfate through a bag opening 28 until the required amount is stored, and packaging to prepare the finished polymeric ferric sulfate.
Use the utility model discloses polymeric ferric sulfate that the device prepared, its index can reach the certified products standard requirement among GB/T14591-2016 "water treatment agent polymeric ferric sulfate", is applicable to the sewage purification treatment at sewage treatment station.

Claims (9)

1. The utility model provides an utilize old and useless battery electrolyte to prepare polymeric ferric sulfate's device, includes electrolyte collecting vessel, ferric sulfate polymerization cauldron and the solid polymeric ferric sulfate storage tank that sets gradually, its characterized in that still includes purification dilute sulfuric acid storage bucket, pressure filter, evaporation enrichment cauldron I, cooling tank I and micro-filter have connected gradually between electrolyte collecting vessel and the purification dilute sulfuric acid storage bucket, be equipped with ferrous sulfate preparation reation kettle between purification dilute sulfuric acid storage bucket and the ferric sulfate polymerization cauldron, ferrous sulfate preparation reation kettle links to each other with evaporation enrichment reation kettle II, cooling tank II and centrifuge in proper order.
2. The device for preparing polymeric ferric sulfate by using the electrolyte of the waste battery according to claim 1, wherein a polymeric ferric sulfate solution storage tank, a polymeric ferric sulfate atomization drying box and a solid polymeric ferric sulfate collection box are sequentially connected between the ferric sulfate polymerization reaction kettle and the solid polymeric ferric sulfate storage tank, the polymeric ferric sulfate atomization drying box is further connected with an air heater, and the solid polymeric ferric sulfate collection box is further connected with a negative pressure fan.
3. The device for preparing polymeric ferric sulfate by using the electrolyte of the waste battery as claimed in claim 2, wherein an oxygen pump inlet, a sodium nitrite solution pump inlet and a feeding port are formed in the ferric sulfate polymerization reaction kettle.
4. The device for preparing the polymeric ferric sulfate by using the electrolyte of the waste battery as claimed in claim 3, wherein a polymeric ferric sulfate solution pump-out pipeline is arranged between the ferric sulfate polymerization reaction kettle and the polymeric ferric sulfate solution storage tank, and the ferric sulfate polymerization reaction kettle and the polymeric ferric sulfate solution storage tank are connected through the polymeric ferric sulfate solution pump-out pipeline.
5. The device for preparing the polymeric ferric sulfate by using the electrolyte of the waste battery as claimed in claim 4, wherein a circulating pipeline is connected to the polymeric ferric sulfate solution pumping-out pipeline in parallel, and the circulating pipeline is simultaneously connected with a polymeric ferric sulfate reaction kettle.
6. The device for preparing polymeric ferric sulfate by using the electrolyte of the waste battery as claimed in claim 5, wherein a pressure gauge is further installed on the ferric sulfate polymerization reaction kettle.
7. The device for preparing the polymeric ferric sulfate by using the electrolyte of the waste battery as claimed in claim 2, wherein a conveying auger I is connected between the solid polymeric ferric sulfate collecting box and the solid polymeric ferric sulfate storage tank, and the solid polymeric ferric sulfate storage tank is provided with a bag opening.
8. The device for preparing polymeric ferric sulfate by using the electrolyte of the waste battery as claimed in claim 1, wherein an electrolyte storage tank is connected between the filter press and the evaporation and enrichment reaction kettle I, and a ferrous sulfate solution storage tank is connected between the ferrous sulfate preparation reaction kettle and the evaporation and enrichment reaction kettle II.
9. The device for preparing the polymeric ferric sulfate by using the waste battery electrolyte as claimed in claim 1, wherein a conveying auger II is connected between the cooling pool II and the centrifuge.
CN202221269431.4U 2022-05-25 2022-05-25 Device for preparing polymeric ferric sulfate by using waste battery electrolyte Active CN218130473U (en)

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